Process of dyeing synthetic polyamide fibers

ABSTRACT

Synthetic polyamide fibers are dyed, at room temperature, with a dyebath containing at least one acid dye dissolved in a medium consisting of water, a lower alkanol having 1 to 4 carbon atoms, and furfuryl alcohol.

United States Patent n91 Arashi 1 1 Aug. 5, 1975 Related U.S. Application Data [63] C0ntinuutinn-in-pzirt of Scr. No. 266,545, June 27.

1972v abandoned.

FOREIGN PATENTS OR APPLICATIONS 1.560.532 1/1968 France 8/173 11171.1)74 6/1967 United Kingdom 8/173 731L763 5/1943 Germany 8/173 OTHER PUBLICATIONS Peters et :11, J. Soc. Dyers & C01 V01. 73. p. 381. March 1958.

Primary E.\.'uminerD0na1d Levy Arm/11c Age/i! or FirmRobert E. Burns; Emmanuel J. Lobato; Bruce L. Adams |52| US. Cl 8/173; 8/41 8; 8/26 51 Int. Cl 4. D06p 1/86 1571 ABSTRACT [581 Field of 8/173, 93 Synthetic Polyamide fibers are y room p ture, with a dycbath containing at least one acid dye [5 References Ci d dissolved in a medium consisting of water, a lower a1- UNITED STATES PATENTS kanol having 1 to 4 carbon atoms, and furfuryl alco- 3.265Afil 8/1966 Luctzcl a a1. 8/84 3.510.243 5/1970 Scurct .4 8/39 13 Claims. 1 Drawing Figure WATER FURFURYL LOWER ALCOHOL ALKANOL CH 3 OH. z s (3 1-1 014,

PATENTEDAUB 5197s 5 9G O 36 WATER FURFURYL LOWER ALCOHOL V ALKANOL CH OH,

PROCESS OF DYEING SYNTHETIC POLYAMIDE FIBERS This is a continuation-in-part of application Ser. No. 266,545, filed June 27, 1972, now abandoned.

The present invention relates to a dyeing process of synthetic polyamidc fibers at room temperature. More particularly it relates to the process of dyeing textile materials containing synthetic polyamide fibers, such as fibers consisting of Nylon 6, Nylon 66, Nylon 9H), Nylon 12, etc, with acid dyes at room temperature.

The term acid dye" as used herein refers to the usual water-soluble acid dye, l l premetallized acid dye, l 2 premctallized acid dye, acid mordant dye, and fluorescent dye and direct dye usable for synthetic polyamide fibers.

Generally speaking, acid dyes, disperse dyes, etc, are used in the dyeing of synthetic polyamide fibers. Usually, acid dyes are widely used because of color fastness, build-up characteristics and costs. In the usual dyeing process of synthetic polyamide fibers, acid dyes are applied to the fibers by dipping them into a dyebath of acid aqueous solution including acid dyes. The dyebath is then heated slowly to a temperature near the boiling point, and maintained at this temperature for a certain time period. Such a dyeing process is applied to the fabric containing synthetic polyamide fibers, with jiggers, beam dyeing equipment, winches and the like.

However, these known methods for the dyeing of fabrics containing synthetic polyamide fibers, have the following disadvantages.

a. Streaks tend to appear on the dyed fabric. Alt htough this problem can be solved by the use of levelling type dyes, such dyes are generally inferior in their wet fastness. Alternatively, so-called milling type dyes and premctallizcd dyes having superior wet fastness can be used, but their practical use is difficult. This difficulty arises because they lack a levcl-dyeing property and, therefore, tend to cause the abovedescribcd streaks on the dyed fabricv b. Color matching is difficult in practice, in that the shade of the color on the product from each batch is often different from the others.

c. The cost of dyeing is considerably increased owing to the low productivity.

(1. Handling of the resulting dyed fabric from each batch is often not uniform.

e. In most cases, ending appears in fabric dyed with jiggers.

In view ofthc above drawbacks, in the present situation of dyeing synthetic polyamide fibers, the inventor has carefully studied new dyeing processes. The object of this study was to improve the efficiency of the dyeing procedure and the quality of the dyed product. As a result of this study, the inventor has accomplished the present invention.

The object of the present invention is to provide a process of dyeing textile materials containing synthetic polyamide fibers by means of which it is possible to dye said fibers at room temperature, without causing faults such as streaks, ending, etc. on the dyed fibers, and moreover, this process has a high productivity.

This object can be accomplished by using the process of the present invention. In this process synthetic polyamidc fibers are treated, at room temperature, with a dyebath containing at least one acid dye dissolved in a medium consisting of water, a lower alkanol having 1 to 4 carbon atoms, such as methyl, ethyl, propyl, isopropyl, butyl and isobutyl alcohols, and furfuryl alco hol.

when applying this process of the present invention to fabric containing synthetic polyamide fibers, the fabric may for example, be dipped into the abovementioned dyebath prepared with a solution of acid dyes and a mixture of water, lower alkanol, and furfuryl alcohol. The fabric may then be nipped evenly to uniformly impregnate the solution into the fabric. Thereafter, the impregnated fabric may be wound and stored at room temperature for a certain time period, e.g. for one night, during which the dyes are fixed into the fabric.

Such a process of dyeing at room temperature is gen erally called a pad-batch method. It is usually used in cases where a fabric of cellulose fibers, such as rayon, cotton, etc., is dyed with an aqueous solution of reactive dyes or direct dyes. However, it has previously not been known that a fabric of synthetic polyamide fibers can be dyed by such pad-batch methods at room temperature. The above process is, however, accomplished by the present invention.

The features of the present invention will be made more apparent by the description set forth in detail hereinafter and by the accompanying drawing.

The process of the invention uses a mixture of water, lower alkanol, and furfuryl alcohol as a dyeing medium in the dyebath. The drawing is a triangular composition diagram for defining the range of mixing ratio in "/0 by volume of the three components of water, lower alkanol and furfuryl alcohol in the medium. Within this range the dyeing according to the process of the present invention is carried out effectively.

From a systematic study by the inventor, it was found that the dyeing according to the process of the present invention is carried out effectively when the mixing ratio of the three components is on or within the quadrilateral ABCD defined in the accompanying drawing.

In the triangular diagram of the drawing, the base represents the mixing ratio of the two components con sisting of furfuryl alcohol and lower alkanol in by volume. On this base side lower alkanol increases from O to 100% as the position moves to the right. The other two sides similarly represent the mixing ratios of water and furfuryl alcohol, and of lower alkanol and water, left and right respectively. That is, the composition of the three components consisting of water, lower alkanol and furfuryl alcohol in by volume is represented by each point within the triangle and the quadrilaterials ABCD as mentioned above. This is defined by coordinates A (watcr 68, lower alkanol 5, furfuryl alcohol 27), B (water 10, lower alkanol 5, furfuryl alcohol C (water (l0, lower alkanol 80, furfuryl alcohol l0) and D (water 43, lower alkanol 47, furfuryl alcohol l0).

In a case where the dyeing medium does not include water at all, the dyed fabric is inferior in the uniformity of the shade of the color and becomes hard. Also the shade of the color is different from those dyed in the usual aqueous dyebath. Additionally, commercially available acid dyes include a certain amount of watersoluble additives such as Glaubers salt, starchy materials, surface active agents, etc. Some of these additives may not be soluble in lower alkanol and furfuryl alcohol. For these reasons, when such commercially available acid dyes are dissolved into lower alkanol and furfuryl alcohol without water. undissolved solids may be disadvantageously separated from the solution. Therefore. the dyeing medium in the dyebath used in the process of the present invention, preferably includes at least l% water.

In a case where the amount of lower alkanol and furfuryl alcohol included in the medium is less than the amount defined by the segment of line AD. the resulting product is inferior in the build-up property of the color and in the uniformity of the color shade. Therefore, the dyeing medium also preferably includes lower alkanol and furfuryl alcohol in amounts not less than that defined by line AD. These alcohols have almost no tendency to decrease such physical properties as tenacity, tearing strength. and abrasion resistance, of synthetic polyamide fibers.

The dyebath used in the process of the present invention should include a sufficient amount of acid such as acetic acid, formic acid, sulfuric acid or hydrochloric acid; together with a desired amount of acid dyes for the bath to be adjusted to the desired value of pH. The pH value may be determined variously, according to the type and concentration of dyes used in the dyebath. In addition, the dyebath used in the process of the invention may, if necessary, include other added auxiliaries such as surface active agents, starchy materials, grape sugar, buffer agents, etc.

One practical use of the process according to the present invention, is that the fabric of synthetic polyamide fibers impregnated with the dyebath, may be wound and stored at room temperature. in addition, textile material of synthetic polyamide fibers may be dyed uniformly by stirring or circulating the dyebath, or by shaking 0r circulating the material, when the material is dipped into the dyebath at room temperature. Alternatively, in a case where the dyeing is carried out in a closed dyeing vessel, the dyebath may be heated slightly in a range that will not cause a decrease in the physical properties of the materials to be dyed.

The features of the process of the present invention are explained in more detail by the following examples.

EXAMPLE 1 i500 m of Nylon 6 taffeta (fabric weight 70 g/m'-) was treated on a pad mangle using the following dyebath:

Nylomine Red A-ZBS (Cl. Acid Red 266) 1.4 kg Furfuryl alcohol 50 l Ethyl alcohol 30 l Water 20 l Acetic acid (SW71) 0.4 l

Wash fastncss JIS [Japanese Industrial Standard) class L- l U45 color decreasing staining to Nylon Light fastncss JIS L-ltM-J Rubbing fastncss S L- (M8 dry These fastness figures were the same as those of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 2 The procedure of Example l was repeated with the following dyebath:

Kayanol Blue NR (KYK. C'.l. Acid Blue I29) 2 Furfuryl alcohol 15 lsopropyl alcohol 25 Water Acetic acid 0.5

The resultant fabric was dyed a bright blue color having the following fastness:

Wash fastness color decreasing class 5 staining to Nylon class 5 Light fastncss class 5 or higher Rubbing fastness dry class 5 wet class 5 EXAMPLE 3 The procedure of Example l was repeated with the following dyebath:

Nylominc Acid Green (Cl. bl57ll] l kg Furfuryl alcohol 4i) i Methyl alcohol 41) 1 Water It) i Acetic acid (80'!!! (1.5

The resultant fabric was dyed a green color having the following fastncss:

Wash fastncss color decreasing class 5 staining to Nylon class 5 Light fzistncss class 5 or higher Rubbing fustncss dry class 5 wet class 5 EXAMPLE 4 1000 m of Nylon 66 twill (fabric weight g/m") was treated on a pad mangle using the following dyeblltlll Tclon Fast Blue ESN (Bayer, (1. Acid Blue 32] 2.5 kg Furfuryl alcohol It] i Methyl alcohol ill I Water 2U l Wash fustncss color decreasing class 5 staining to Nylon class 5 Light fastncss class 6 Rubbing fastncss dry class 5 wet class 5 There was no difference between these fastness figarcs and those of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 5 1500 m of Nylon 6 taffeta (fabric weight 70 g/m) was treated by the procedure as described in Example 1 with the following dyebath:

(.l. Acid Yellow H9 L5 kg Methyl alcohol K l Furfuryl alcohol H) l Water I0 I Acetic acid (80%) l The resultant fabric was dyed a yellow-brown color and the dyeing fastness was the same as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 6 1000 m of Nylon 6 twill (fabric weight 150 g/m") was treated by the procedure as described in Example 4, except that the wet pick up was 65%. with the following dyebath:

(4]. Acid Red 257 L3 kg (.l. Acid Orange 67 0.8 kg (.l. Acid Blue I29 0.4 kg Furfuryl alcohol 85 l n-Butyl alcohol 1 Water l Acetic acid (80')? l l l The resultant fabric was dyed a rubinc-red color and the dyeing fastness was the same as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 7 [500 m of Nylon 6 nonwoven fabric (fabric weight 50 g/m was treated on a pad mangle using the following dyebath:

Cl. Direct Red l l kg Furfuryl alcohol l0 1 Ethyl alcohol 47 l Water 43 Acetic acid (809; l

EXAMPLE 8 [000 m of Nylon 6 tricot knot fabric (fabric weight I g/m) was treated on a pad mangle using the following dycbath:

(.l. Flourcsccnt 90 0.5 kg Furfuryl alcohol 27 l lsn-butyl alcohol 5 l Water 68 l Acetic acid (80%] 0.5 l

The wet pick up on the padded fabric was 80%. The fabric was then stored at room temperature for 16 hours on a rotating roller with a polyethylene sheet cover. Then. the fabric impregnated with the dyebnth was washed with water and dried.

The fabric was dyed a white color having the same fastness as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 9 I000 m of Nylon 66 satin crepe (fabric weight l 10 g/m) was treated on a pad mangle using the following dyebath:

C.l. Acid Blue ll3 C.l. Acid Red 266 CI. Acid Yellow 64 Furfuryl alcohol lso-propyl alcohol 40 l Water [(1 l Acetic acid I l PP. COMO The wet pick up on the padded fabric was 80%. The fabric was then stored at room temperature for 20 hours on a rotating roller with a polyethylene sheet cover. Then the fabric impregnated with the dyebath was washed with water and dried.

The fabric was dyed a navy blue color having the same fastness as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 10 1000 m of Nylon 6 dobby cloth (fabric weight l00 glm was treated on a pad mangle using the following dyebath:

Cil. Acid Red 314 1.8 kg Furfuryl alcohol 45 l Propyl alcohol 5 l Water 50 l Acetic acid (80% l The wet pick up on the padded fabric was 70%. The fabric was then stored at room temperature for 18 hours on a rotating roller with a polyethylene sheet cover. Then, the fabric impregnated with the dyebath was washed with water and dried.

The fabric was dyed a rubine-rcd color having the same fastness as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 1 l 1000 m of Nylon 6 satin (fabric weight l20 glm' was treted on a pad mangle using the following dyebath:

Cl. Direct Blue 0.5 kg Cl. Direct Yellow 44 0.5 kg Furfuryl alcohol I0 I Methyl alcohol 65 l Water 25 l Acetic acid (80% l The wet pick up on the padded fabric was 80 The fabric was then stored at room temperature for 24 hours on a rotating roller with a polyethylene sheet cover. Then. the fabric impregnated with the dyebath was washed with water and dried.

The fabric was dyed a yellowish-green color having the same fastness as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

EXAMPLE 12 1000 m of Nylon 66 tropical (fabric weight 100 g/m") was treated on a pad mangle using the following dyebath:

Cl. Acid Blue 183 [.2 kg C]. Acid Yellow I27 I kg Furfuryl alcohol l l Ethyl alcohol 35 l Water 51) l Acetic acid (807: l l l The wet pick up on the padded fabric was 7571. The fabric was then stored at room temperature for 20 hours on a rotating roller with a polyethylene sheet cover. Then, the fabric impregnated with the dyebath was washed with water and dried.

The fabric was dyed a green color having the same fastness as that of the color of a fabric dyed by the usual process of dyeing with a boiled aqueous dyebath.

What I claim is:

l. A process of dyeing synthetic polyamide fibers comprising treating synthetic polyamide fibers. at room temperature. with a dyebath containing at least one acid dye dissolved in a medium consisting of water, lower alkanol having 1 to 4 carbon atoms, and furfuryl alcohol in a composition by volume on or within a quadrilateral, in a triangular composition diagram. defined by the following coordinates:

A. (water 68. lower alkanol 5, furfuryl alcohol 27).

B. (water l0, lower alkanol 5, furfuryl alcohol 85),

C. (water 10, lower alkanol 80, furfuryl alcohol and D. (water 43, lower alkanol 47, furfuryl alcohol 10).

2. A process as claimed in claim 1, wherein said medium consists of 607: water, 25% isopropyl alcohol and l5Z' furfuryl alcohol. 1

3. A process as claimed inclaim 1, wherein said me dium consists of 20?! water, methyl alcohol and [U71 furfuryl alcohol.

4. A process as claimed in claim 1, wherein said medium consists of 20% water, 40% methyl alcohol and 40% furfuryl alcohol.

5. A process as claimed in claim 1. wherein said medium consists of 20% water. 30% ethyl alcohol and 509: furfuryl alcohol.

6. A process as claimed in claim I, wherein said medium consists of 1071 water, methyl alcohol and 10% furfuryl alcohol.

7. A process as claimed in claim I, wherein said medium consists of.l0% water. 5% n-butyl alcohol and furfuryl alcohol.

8. A process as claimed in claim I, wherein said medium consists of 43% water. 47% ethyl alcohol and 10% furfuryl alcohol.

9. A process as claimed in claim 1,.wherein said medium consists f 68% water. 5% iso-butyl alcohol and 27% furfuryl alcohol. 1

10. A process as claimed in claim I, wherein said medium consists of [0% water. 40% iso-propyl alcohol and 50% furfuryl alcohol.

1 l. A process as claimed in claim I, wherein said medium consists of 50% water 5% propyl alcohol and 45% furfuryl alcohol.

12. A process as claimed in claim I, wherein said medium consists of 25% water. 65% methyl alcohol and 1071 furfuryl alcohol.

13. A process as claimed in claim I, wherein said medium consists 'of 50% water; 35% ethyl alcohol and 15% furfuryl 'alcohol.

wiriqm 

1. A PROCESS OF DYING SYNTHETIC POLYMIDE FIBERS COMPRISING TREATING SYNTHETIC POLYMIDE FIBERS, AT ROOM TEMPERATURE, WITH A DYEBATH CONTAINING AT LEAST ONE ACID DYE DISSOLVED IN A MEDIUM CONSISTING OF WATER, LOWER ALKANOL HAVING 1 TO 4 CARBON ATOMS, AND FURFURYL ALCOHOOL IN A COMPOSITION BY VOLUME ON OR WITHIN A QUADRILATERAL, IN A TRIANGULAR COMPOSITION DIAGRAM, DEFINED BY THE FOLLOWING CO-ORDINATES: A. (WATER 68, LOWER ALKANOL 5, FURFURYL ALCOHOL 27), B. (WATER 10, LOWER ALKANOL 5, FURFURYL ALCOHOL 85), C. (WATER 10, LOWER ALKANOL 80, FURFURYL ALCOHOL 10), AND D. (WATER 43, LOWER ALKANOL 47, FURFURYL ALCOHOL 10).
 2. A process as claimed in claim 1, wherein said medium consists of 60% water, 25% isopropyl alcohol and 15% furfuryl aLcohol.
 3. A process as claimed in claim 1, wherein said medium consists of 20% water, 70% methyl alcohol and 10% furfuryl alcohol.
 4. A process as claimed in claim 1, wherein said medium consists of 20% water, 40% methyl alcohol and 40% furfuryl alcohol.
 5. A process as claimed in claim 1, wherein said medium consists of 20% water, 30% ethyl alcohol and 50% furfuryl alcohol.
 6. A process as claimed in claim 1, wherein said medium consists of 10% water, 80% methyl alcohol and 10% furfuryl alcohol.
 7. A process as claimed in claim 1, wherein said medium consists of 10% water, 5% n-butyl alcohol and 85% furfuryl alcohol.
 8. A process as claimed in claim 1, wherein said medium consists of 43% water, 47% ethyl alcohol and 10% furfuryl alcohol.
 9. A process as claimed in claim 1, wherein said medium consists of 68% water, 5% iso-butyl alcohol and 27% furfuryl alcohol.
 10. A process as claimed in claim 1, wherein said medium consists of 10% water, 40% iso-propyl alcohol and 50% furfuryl alcohol.
 11. A process as claimed in claim 1, wherein said medium consists of 50% water, 5% propyl alcohol and 45% furfuryl alcohol.
 12. A process as claimed in claim 1, wherein said medium consists of 25% water, 65% methyl alcohol and 10% furfuryl alcohol.
 13. A process as claimed in claim 1, wherein said medium consists of 50% water, 35% ethyl alcohol and 15% furfuryl alcohol. 